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Separation method of aldehyde/alcohol mixture

A separation method and mixture technology are applied in the separation field of butyraldehyde and ethanol mixture, which can solve the problems of increasing the difficulty and cost of waste disposal, increasing the consumption of butyraldehyde of raw materials, and being difficult to realize the recycling of butyraldehyde, so as to achieve the realization of recycling and reuse. The effect of resource utilization and reduction of three wastes

Active Publication Date: 2017-12-01
JIANGSU YANGNONG CHEM GROUP +2
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

Since the boiling point difference between butyraldehyde and ethanol is only 2-3°C, it is impossible to obtain butyraldehyde with a content of more than 99% by direct rectification, and it is difficult to realize the recycling of butyraldehyde
Therefore, the traditional process directly treats it as waste, which not only increases the consumption of raw material butyraldehyde, but also increases the difficulty and cost of waste treatment
In the prior art, extraction and rectification are used for separation, and the content of butyraldehyde after separation is generally less than 90%, which cannot meet the requirements of the Prins reaction

Method used

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  • Separation method of aldehyde/alcohol mixture
  • Separation method of aldehyde/alcohol mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Adopt Corning G1 microchannel reactor, use 8 plates, the volume of every plate is 8.4ml, and total volume is 67.2ml, feeds raw material solution (the quality of butyraldehyde and ethanol) respectively to the first plate with three advection pumps ratio is 3:1), benzene and water, the mass flow rates of the three are 10g / min, 10g / min and 40g / min respectively, and the residence time is about 63s. After running for 10 minutes, 176.0 g of oil phase and 423.6 g of water phase were obtained after passing through the stratifier, wherein the relative content of butyraldehyde in the oil phase was 98.6% (calculated after deducting benzene). The direct distillation of the oil phase obtains about 72.81g of 99% butyraldehyde, the recovery rate of butyraldehyde is about 96.1%, and recycling of benzene is used; the content of ethanol in the water phase is about 5.85%, and the butyraldehyde is about 0.03%, and the direct distillation obtains 25.86% of 95% ethanol g, the ethanol recover...

Embodiment 2

[0020] Adopt Corning G1 microchannel reactor, use 8 plates, the volume of every plate is 8.4ml, and total volume is 67.2ml, feeds raw material solution (the quality of butyraldehyde and ethanol) respectively to the first plate with three advection pumps ratio of 4:1), n-butyl acetate and water, the mass flow rates of the three are 12g / min, 9g / min and 35g / min respectively, and the residence time is about 67s. After running for 10 minutes, 188.1 g of oil phase and 371.2 g of water phase were obtained after passing through the stratifier, wherein the relative content of butyraldehyde in the oil phase was 98.7% (calculated after deducting n-butyl acetate). The direct rectification of the oil phase obtains about 93g of 99% butyraldehyde, and the recovery rate of butyraldehyde is about 95.9%. The recovery of n-butyl acetate is recycled; the ethanol content in the water phase is about 6.42%, and the butyraldehyde is about 0.02%. 24.9g of 95% ethanol, the ethanol recovery rate is abou...

Embodiment 3

[0022] Compared with Example 1, no auxiliary agent is introduced in the water washing. Adopt Corning G1 microchannel reactor, use 8 plates, the volume of each plate is 8.4ml, and total volume is 67.2ml, feeds raw material solution (the quality of butyraldehyde and ethanol) respectively to the first plate with three advection pumps The ratio is 3:1) and water, the mass flow rates of the two are 10g / min and 40g / min respectively, and the residence time is about 77s. After a total of 10 minutes of operation, 82.6g of the oil phase and 416.8g of the water phase were obtained after passing through the stratifier. The relative content of butyraldehyde in the oil phase was 86.7%, and 99% of butyraldehyde could not be obtained by direct distillation of the oil phase; the ethanol content in the water phase was 3.6% , the butyraldehyde content is 2.51%, and direct distillation cannot obtain 95% ethanol equally.

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Abstract

The invention relates to a separation method of an aldehyde / alcohol mixture. The invention provides the solving scheme as follows: a butyraldehyde / ethyl alcohol mixed solution is taken as a raw material; butyraldehyde is effectively separated from ethyl alcohol by adopting a corning G1 microchannel reactor through a process of adding a third-party assistant for washing, and the butyraldehyde with the content of 99% and industrial ethyl alcohol with the content of 95% are finally obtained, and therefore, resource utilization of a liquid waste is achieved, so that the butyraldehyde can be recycled and the raw material cost is reduced.

Description

technical field [0001] The invention relates to a method for separating butyraldehyde and ethanol mixture. Background technique [0002] After the Prins reaction and hydrolysis reaction of n-butyraldehyde and vinyl ethyl ether, the reaction solution contains a mixture of butyraldehyde and ethanol, wherein the mass ratio of butyraldehyde to ethanol is about 3-4:1. The specific process can be found in CN106380383. Since the boiling point difference between butyraldehyde and ethanol is only 2-3°C, it is impossible to obtain butyraldehyde with a content of more than 99% by direct rectification, and it is difficult to realize the recycling of butyraldehyde. Therefore, the traditional process directly treats it as waste, which not only increases the consumption of raw material butyraldehyde, but also increases the difficulty and cost of waste treatment. In the prior art, extractive distillation is used for separation, and the content of butyraldehyde after separation is generally...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/02C07C45/82C07C31/08C07C29/80B01J19/00
CPCB01J19/0093C07C29/80C07C45/82C07C47/02C07C31/08
Inventor 丁克鸿徐林孙诚李明马庆炎王敏娟邹爱宗
Owner JIANGSU YANGNONG CHEM GROUP
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